EP2574922A1 - Vorrichtung zur Bestimmung der Menge von flüchtigen Unreinheiten in einem flüssigen Material und Verfahren zur Verwendung davon - Google Patents

Vorrichtung zur Bestimmung der Menge von flüchtigen Unreinheiten in einem flüssigen Material und Verfahren zur Verwendung davon Download PDF

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Publication number
EP2574922A1
EP2574922A1 EP11183136A EP11183136A EP2574922A1 EP 2574922 A1 EP2574922 A1 EP 2574922A1 EP 11183136 A EP11183136 A EP 11183136A EP 11183136 A EP11183136 A EP 11183136A EP 2574922 A1 EP2574922 A1 EP 2574922A1
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EP
European Patent Office
Prior art keywords
measuring
liquid material
measuring chamber
chamber
volatile impurities
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP11183136A
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English (en)
French (fr)
Inventor
Erik Grove-Nielsen
Erik Wolf
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Siemens AG
Original Assignee
Siemens AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Siemens AG filed Critical Siemens AG
Priority to EP11183136A priority Critical patent/EP2574922A1/de
Publication of EP2574922A1 publication Critical patent/EP2574922A1/de
Withdrawn legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; Plastics; Rubber; Leather

Definitions

  • the invention relates to an apparatus for determining the amount of volatile impurities in a liquid material and to a method for using the same.
  • VARTM vacuum assisted resin transfer moulding
  • Air voids or other gas voids are released in the uncured resin at low pressure which leads to lower physical strength and lower overall quality of the final component, which in turn necessitates costly repair and refinishing work.
  • the apparatus for determining the amount of volatile impurities in a liquid material comprises a measuring chamber with a bottom part, a chamber part and a measuring part.
  • the bottom part is connected to the chamber part which in turn is connected to the measuring part such that these parts enclose the measuring chamber.
  • the measuring part comprises a closable opening for introducing a liquid material having volatile impurities into the measuring chamber.
  • the measuring chamber further comprises one or more transparent panels for devising the processes going on in the measuring chamber and in particular, for measuring a gas volume resulting from gas bubbles released over a free surface of the liquid material.
  • a measuring scale may be arranged at the one or more transparent panels.
  • the measuring chamber comprises a bottom part which is moveably arranged in the chamber part and configured to reduce the pressure in the measuring chamber to a predefined pressure such that the volatile impurities are released from the liquid material as gas bubbles.
  • this apparatus comprises built-in means to reduce the pressure in the measuring chamber. Therefore, it is not necessary to connect an external vacuum generator to the measuring chamber and the pressure in the measuring chamber may be reduced manually. Hence, the apparatus is effective and nevertheless cost-efficient and robust.
  • the measuring part comprises a tubular part and the chamber part comprises a cone-shaped part.
  • these parts may have other shapes, a tubular measuring part and an at least partly cone-shaped chamber part allow for determining the amount of volatile impurities more precisely. This is because the cone-shaped form supports assembling and rising of gas bubbles released from the liquid material and the tubular form of the measuring part facilitates the measurement of a gas volume in the measuring chamber.
  • the chamber part may further comprise a cylindrical part and the moveable bottom part may comprise an inner piston part, an outer piston part and a control fluid having a vapor pressure, wherein the control fluid is arranged between the inner piston part and the outer piston part in the cylindrical part of the measuring chamber.
  • These parts form a cylinder piston system, wherein the inner piston part is guided axially slidable relative to the outer piston part within the chamber part as long as the pressure in the measuring chamber is above the vapor pressure of the control fluid. That means, the control fluid is chosen such that the vapor pressure of the control fluid corresponds to the pressure intended in the measuring chamber for releasing of volatile impurities from the liquid material. Thus, a predefined constant pressure may be maintained in the measuring chamber.
  • a method for using the apparatus comprises the steps of filling the measuring chamber completely with a liquid material comprising volatile impurities, closing the measuring chamber hermetically sealed, reducing the pressure in the measuring chamber to a predefined pressure such that the volatile impurities are released over a free surface of the liquid material as gas bubbles, maintaining the predefined pressure in the measuring chamber for a predetermined time such that the gas bubbles collapse leaving a gas volume, and measuring the gas volume which indicates the amount of volatile impurities in the liquid material.
  • the measuring chamber is completely filled with the liquid material. This also ensures unchanged measurement conditions when measuring a series of liquid material samples or different liquid materials. Hence, the results of these measurements may be compared easily.
  • the liquid material may comprise a liquid plastic material for instance a polymeric material like a thermosetting polymer.
  • the method may be applied in a production process of fiber reinforced composite components to evaluate the quality of a polymer melt prior to a casting process.
  • a polymer material of a lower quality may be identified and rejected which enhances the quality of the final composite component.
  • the overall production costs are reduced, which is especially advantageous in case of expensive and laborious processes, for instance casting processes of wind turbine rotor blades.
  • liquid material may be heated in the measuring chamber to reduce the viscosity of the liquid material in order to facilitate releasing of gas bubbles.
  • Volatile impurities in a liquid polymer comprise gaseous components, for instance trapped air.
  • the volatile impurities may comprise liquid components which volatilize, if the material is exposed to a vacuum, i.e. to a pressure which is below the atmospheric pressure of 1000 mbar. This happens for instance during a casting process of a composite component.
  • An example of such a liquid component in this context is a reactive diluent in an epoxide resin.
  • the apparatus 22 is preferably portable and comprises a hermetically sealable measuring chamber 8 with a bottom part 5, a chamber part 6 and a measuring part 7, wherein the bottom part 5 is connected to the chamber part 6 and the chamber part 6 is connected to the measuring part 7.
  • the chamber part 6 comprises a cylindrical part and cone-shaped part.
  • a tapered end 6a of the cone-shaped part 6 is connected to an end 7a of the measuring part 7, wherein the measuring part 7 is tubular.
  • the opposite end of the cone-shaped part is connected to the cylindrical part.
  • An inlet opening 1 is arranged in the tubular measuring part 7, preferably, at a free end of this tubular measuring part 7.
  • the inlet opening 1 is used to introduce a liquid material 11 into the measuring chamber 8.
  • the inlet opening 1 is used to discharge the liquid polymer 11 from the measuring chamber 8 after having measured the amount of volatile impurities.
  • the inlet port 1 comprises a valve 4, for instance a magnetic valve or other means suitable for closing the measuring chamber 8 hermetically.
  • the measuring chamber 8 comprises a bottom part 5 which is moveably arranged in the chamber part 6.
  • the moveable bottom part 5 is configured to reduce the pressure in the measuring chamber 8 by being moved in such a way that the volume of the measuring chamber 8 increases.
  • the pressure in the measuring chamber 8 may be reduced by moving the moveable bottom part 5 in a direction away from the tubular measuring part 7.
  • the moveable bottom part 5 comprises an inner piston part 5a, an outer piston part 5b and a control fluid 18 having a defined gas pressure.
  • This control fluid 18 is arranged between the inner piston part 5a and the outer piston part 5b.
  • a first sealing 13a is arranged between the inner piston part 5a and the chamber part 6 and a second sealing 13b is arranged between the outer piston part 5b and the chamber part 6.
  • the inner piston part 5a is guided within the chamber part 6 in an axially slidable manner relative to the outer piston part 5b.
  • the control fluid stiffly connects the inner piston part 5a and the outer piston part 5b.
  • Vapor pressure means a substance and temperature depending gas pressure and denotes the ambient pressure, below which a fluid starts vaporizing at a constant temperature.
  • control fluid 18 starts boiling, if the intended predefined pressure is reached in the measuring chamber 8. If the outer piston 5b is further moved away from the inlet opening 1, the inner piston part 5a will no longer follow and the pressure in the measuring chamber 8 will not be reduced any further. As a result, a predefined constant pressure is generated within the measuring chamber 8.
  • a rod 19 and/or a handle 20 may be connected to the moveable bottom part 5 to faciltate moving of the bottom part 5.
  • a transparent panel 9 is arranged in the tubular measuring part 7 for observing at least a part of the measuring chamber 8.
  • a further transparent panel may be arranged in the chamber part 6 for monitoring the processes going on in the measuring chamber 8.
  • the transparent panel 9 and/or the further transparent panel may be configured as a window of any shape and may include any transparent material, for instance glass or acryl glass.
  • the tubular measuring part 7 and/or the chamber part 6 may be made of a transparent material for observing the inside of the measuring chamber 8.
  • a measuring scale 10 is arranged at the transparent panel 9.
  • the measuring chamber 8 comprises a heating device (not shown) for heating the liquid polymer 11 in the measuring chamber 8 to reduce the viscousity thereof.
  • the heating device may, for instance, comprise a battery-powered heating coil connected to the chamber part 6.
  • the measuring chamber 8 may be made, at least partly, of a metallic material, for instance aluminium, high-grade steel or copper, in order to facilitate the heat transfer from the heating device to the liquid polymer 11 in the measuring chamber 8.
  • a metallic material for instance aluminium, high-grade steel or copper
  • the moveable bottom part 5 is moved to suck the liquid material from a container into the measuring chamber 8.
  • the liquid polymer material for instance an epoxide resin, is introduced through the inlet opening 1.
  • the apparatus 22 is turned such that the tubular measuring part 7 faces upwards. Air which has been kept in the measuring chamber 8 is discharged or pressed out through the inlet opening 1. Thus, the measuring chamber is filled completely.
  • the measuring chamber is then closed hermetically using a valve 4 connected to the inlet opening 1, wherein "hermetically” or “hermetically sealed” means leak-proof and vacuum tight.
  • the moveable bottom part 5 After having closed the measuring chamber, the moveable bottom part 5 is moved by pulling the rod 19 downwards, as indicated by an arrow in FIG 2b . That means the rod 19 and thus, the moveable bottom part 5, is pulled in a direction away from the inlet opening 1. Thereby, the pressure in the measuring chamber 8 is reduced to a predefined pressure such that the volatile impurities are released from the liquid polymer 11 as gas bubbles 12.
  • the control fluid 18 starts boiling at the predefined pressure intended in the measuring chamber 8 for the bubble 12 formation and for the measurement of the remaining gas volume in the measuring chamber 8. If this pressure is reached, the inner piston part 5a does not move any further and the pressure in the measuring chamber 8 remains constant. Gas bubbles 12 in the liquid material expand, migrate into other gas bubbles, assemble and rise upwardly. The gas bubbles 12 are released over a free surface of the liquid polymer 11 in the measuring chamber and a gas bubble column 17 builds-up in the tubular measuring part 7.
  • the predefined pressure is maintained for a predetermined time. Finally, the gas bubbles collapse.
  • the gas bubble column 17 disappears leaving a certain gas volume in the tubular measuring part 7.
  • the gas volume is observable as a "free" or transparent gas column 24. This involves a remaining filling level of the measuring chamber 8 which is reduced compared to the filling level at the beginning of the measuring procedure. This remaining filling level or the height of the transparent gas column 24 may be read off by means of the transparent panel 9 having a measuring scale 10 printed thereon.
  • the gas volume is measured after a predetermined time which may also be referred to as waiting time.
  • the predetermined time depends on the liquid material 11 to be evaluated and on of the temperature of the liquid material 11.
  • a waiting time of a few minutes may be sufficient, wherein at a temperature of about 20 degrees Celsius a waiting time of about one hour could be required.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
EP11183136A 2011-09-28 2011-09-28 Vorrichtung zur Bestimmung der Menge von flüchtigen Unreinheiten in einem flüssigen Material und Verfahren zur Verwendung davon Withdrawn EP2574922A1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP11183136A EP2574922A1 (de) 2011-09-28 2011-09-28 Vorrichtung zur Bestimmung der Menge von flüchtigen Unreinheiten in einem flüssigen Material und Verfahren zur Verwendung davon

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP11183136A EP2574922A1 (de) 2011-09-28 2011-09-28 Vorrichtung zur Bestimmung der Menge von flüchtigen Unreinheiten in einem flüssigen Material und Verfahren zur Verwendung davon

Publications (1)

Publication Number Publication Date
EP2574922A1 true EP2574922A1 (de) 2013-04-03

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP11183136A Withdrawn EP2574922A1 (de) 2011-09-28 2011-09-28 Vorrichtung zur Bestimmung der Menge von flüchtigen Unreinheiten in einem flüssigen Material und Verfahren zur Verwendung davon

Country Status (1)

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EP (1) EP2574922A1 (de)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5285674A (en) * 1991-06-18 1994-02-15 Spuhl Ag Measurement device for detecting gas charge of a plastic component
US5442948A (en) * 1991-04-01 1995-08-22 The United States Of American As Represented By The Secretary Of The Navy Apparatus and method for determining amount of gases dissolved in liquids
EP0866328A1 (de) * 1997-03-14 1998-09-23 Stücklin & Cie AG Vorrichtung zur Messung des Gasgehalts von Flüssigkeiten
US6082174A (en) * 1998-08-11 2000-07-04 Benchtop Machine And Instrument, Inc. Apparatus and method for determining the amount of entrapped gas in a material
US20050092062A1 (en) * 2003-10-30 2005-05-05 Bayer Aktiengesellschaft Device and method for determining the gas content of a liquid
DE102005025382B3 (de) * 2005-05-31 2007-02-08 Burger Wärmetechnik GmbH Verfahren und Vorrichtung zur Bestimmung von freiem und gelöstem Gas in Wasser

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5442948A (en) * 1991-04-01 1995-08-22 The United States Of American As Represented By The Secretary Of The Navy Apparatus and method for determining amount of gases dissolved in liquids
US5285674A (en) * 1991-06-18 1994-02-15 Spuhl Ag Measurement device for detecting gas charge of a plastic component
EP0866328A1 (de) * 1997-03-14 1998-09-23 Stücklin & Cie AG Vorrichtung zur Messung des Gasgehalts von Flüssigkeiten
US6082174A (en) * 1998-08-11 2000-07-04 Benchtop Machine And Instrument, Inc. Apparatus and method for determining the amount of entrapped gas in a material
US20050092062A1 (en) * 2003-10-30 2005-05-05 Bayer Aktiengesellschaft Device and method for determining the gas content of a liquid
DE102005025382B3 (de) * 2005-05-31 2007-02-08 Burger Wärmetechnik GmbH Verfahren und Vorrichtung zur Bestimmung von freiem und gelöstem Gas in Wasser

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